CN103951290B - A kind of high-heat resistance shock resistant calcium oxide pelletizing and preparation method - Google Patents
A kind of high-heat resistance shock resistant calcium oxide pelletizing and preparation method Download PDFInfo
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Abstract
A kind of high-heat resistance shock resistant calcium oxide pelletizing and preparation method, Ca (OH)
2it is 60.0-150.0 μm that content is milled to granularity at the carbide slag powder of 91.0-94.0%; Add the H of 5.0-15.0%
2o mixes as binding agent; By the powder of mixing at 100.0-350.0kgf/cm
2forming pressure under compression moulding pressurize 0.5-3.0min; Dry 10.0-24.0h; By dried base substrate at CO
2concentration is be fired to 450.0-650.0 DEG C, constant temperature 15.0-45.0min under the atmosphere of 10.0-25.0%; Furnace cooling calcine 90.0-120.0min in 900.0-1150.0 DEG C of temperature range after.Calcium oxide pelletizing prepared by the present invention is being 500.0-1100.0 DEG C with the room temperature temperature difference, cold cycling 5.0-10.0 strength degradation 6.0-25.0%.Method of the present invention improves calcium oxide pelletizing at the heat-shock resistance utilizing two stages of process: be cooled to the chilling of 100-200 DEG C to impact from 1100-1200 DEG C after calcined by rotary kiln completes; By the anxious thermal shocking of room temperature to 1000.0 DEG C during input furnace of calcium carbide.The present invention simultaneously efficiently dissolves and has processed carbide slag, has higher environmental benefit and economic benefit.
Description
Technical field
The present invention relates to large Industrial Solid Waste application technology as the second resource field, one utilizes carbide slag to prepare high-heat resistance shock resistant calcium oxide pelletizing and preparation method.
Background technology
Carbide slag produces the one that gives off in acetylene process with Ca (OH) in calcium carbide process PVC
2for main component and the industrial residue of the process that is difficult to dissolve.Ca (OH)
2content can reach 80.0-90.0%, has very large potential resources recycle value, can separation, impurity removal reshaping SINTERING PRODUCTION calcium oxide, produces calcareous raw material cycling and reutilization as calcium carbide.
During calcium carbide is produced, use calcium oxide pelletizing as calcium carbide raw materials for production comparatively powdery calcium oxide be convenient to product C O and discharge, promote that reaction is carried out, and the high porosity of highly active calcium oxide pelletizing effectively facilitates the carrying out of solid-solid reaction transmittance process, significantly improves the response capacity with coke.Heat-shock resistance refers to that the temperature that material bears to a certain degree sharply changes and the unlikely destroyed performance of structure, but calcium oxide pelletizing is embodied in the requirement of heat-shock resistance in following two utilizing in process: on the one hand calcium oxide pelletizing when entering calcined by rotary kiln in stand thermal shocking and the chilling impact of cooling air after calcine of the high-temperature atmosphere of 900.0-1100.0 DEG C produced from coal dust firing, calcium oxide pelletizing easily bursts efflorescence, this will cause " ring formation " of rotary kiln, significantly reduce kiln work-ing life; If the anxious thermal shocking generation thermal spalling standing about 1000.0 DEG C, electric arc furnace top when calcium oxide pelletizing drops into furnace of calcium carbide by room temperature on the other hand will greatly reduce the response capacity of pelletizing and coke.Therefore, preparation has excellent thermal shock resistance calcium oxide pelletizing is the technical barrier that carbide slag recycle solves as carbide raw material an urgent demand.Calcium oxide pelletizing prepared by the present invention is being 500.0-1100.0 DEG C with the room temperature temperature difference, cold cycling 5.0-10.0 strength degradation 6.0-25.0%
By retrieval, do not retrieve the correlation technique patent about utilizing carbide slag to prepare high-heat resistance shock resistant calcium oxide pelletizing.CN1159795 discloses a kind of Li
2onAl
2o
3mSiO
2matter low expansion ceramic and manufacture method thereof, by adding 9.0-12.0% industrial lithium carbonate, 49.0-52.0% kaolin, 37.0-39.0% quartz is ceramic matrix raw material, adds 0.5-2.0% germanium oxide and prepares as sintering aids low-expansion sosoloid that principal crystalline phase is petalite.CN88100211 discloses a kind of preparation method of high-strength shock resistant heat insulating porous ceramic, the method obtains the mullite ball milling that purity is greater than 98.4% mullite powder that granularity is less than 1.0 μm, then with the zirconium hydroxide adopting coprecipitation method to prepare and yttrium hydroxide mixed sols mixing granulation, first dry-pressing formed hydrostatic profile is again adopted to be fired into high-strength shock resistant heat insulating porous ceramic.CN103351116A discloses a kind of preparation method of material of energy-saving type high temperature-resisting high-heat resistance shock resistant, and the method is introduced the blank microstructure of this based article of trace rare earth oxides moderate control and improved heat conductivility to increase substantially its thermal shock resistance in its base substrate.CN101805201A discloses a kind of preparation method of porous silicon carbide ceramics with high thermal shock resistance, the method with silicon-resin core shell structure precursor powder, aluminum oxide, silicon-dioxide and yttrium oxide according to quality than scope for 100.0:(0.5-10.0): (0.1-5.0) mix, mixed powder after pressure forming, charing process and sintering processes, obtains porous silicon carbide ceramics with high thermal shock resistance again.
Comprehensive foregoing invention, mainly there is following deficiency in existing invention: how (1) existing invention improves the thermal shock resistance of material monolithic mutually by introducing low bulk, the harm that hotchpotch may cause kiln; (2) existing invention unilaterally can only improve thermal shock resistance or improve intensity, lacks a kind of comprehensive regulation not only having had high reactivity but also had high strength.
Summary of the invention
The technology of the present invention is dealt with problems: overcome the deficiencies in the prior art, poor for calcium oxide pelletizing heat-shock resistance, be easy to the technical barrier of explosion efflorescence after the match through heat-shock at alternating temperature-changing, a kind of high-heat resistance shock resistant calcium oxide pelletizing and preparation method are provided, Regulation Mechanism of the present invention is the porous CaO pelletizing weave construction by changing after calcining: pore structure, porosity, pore distribution improve the thermal conductivity of calcium oxide pelletizing, thus improves pelletizing heat-shock resistance.
The principle of concrete grammar of the present invention is: carry out technological design from the pre-treatment of pelletizing powder, pelletizing compression moulding, pelletizing calcining three phases, obtain the parameter area that can improve calcium oxide pelletizing heat-shock resistance.This regulate and control method is according to being following three processes: in powder preprocessing process, by changing the weave construction of carbide slag grain graininess proportioning regulation and control carbide slag particle packing mode control calcium oxide calcining metapore; In cold pressure procedure, changing bonding state between powder by changing compacting system and binder amount, being not only conducive to improving intensity but also being conducive to acceleration of sintering making calcium oxide pelletizing obtain even porous mechanism; Calcination process changes sintering schedule and calcium oxide crystal appropriateness is grown up, form the through-hole structure that porosity is high, pore distribution is even, aperture is suitable, effective raising thermal conductivity, is conducive to the large hot-fluid in local and disperses, effectively reduce thermal stresses thus improve calcium oxide pelletizing heat-shock resistance.Another innovative point of the present invention is in-situ preparation pore-forming material: present method does not introduce pore-forming material, make use of calcium hydroxide to calcine in carbon dioxide atmosphere easily and carbon dioxide reaction generates the unstable characteristic of calcium carbonate, utilize the calcium carbonate original position of carbonization to produce pore-forming material, in decomposition course, produce carbon dioxide to overflow the pore that formation can be made a large amount of.The calcium carbonate dosage of pore-creating is controlled by the constant temperature time in calcium hydroxide decomposition temperature section.Calcium oxide pelletizing pore structure and grain growing is made to coordinate to be an optimum value finally by the sintering temperature and sintering time that regulate and control calcination of calcium carbonate process, obtain the calcium oxide pelletizing with high-heat resistance shock resistant, be recycling in calcium carbide to produce, turn waste into wealth, have very big economy and environment effect.
The technology of the present invention solution: a kind of high-heat resistance shock resistant calcium oxide pelletizing and preparation method, as shown in Figure 1, comprise the following steps:
(1) by Ca (OH)
2it is 60.0-150.0 μm that the carbide slag powder that purity is greater than 91.0-94.0% is milled to granularity, and the weight proportion between three kinds of carbide slag grain graininess is: (60-90 μm: 90-120 μm: 120-150 μm) is respectively (4-6:2-4:2-4).Calcium oxide pelletizing heat-shock resistance increases with carbide slag powder granularity and reduces.
(2) H of 5.0-15.0% will be added in carbide slag powder pretreated in described step (1)
2o is as binding agent and mix, and calcium oxide pelletizing heat-shock resistance increases with water add-on and improves.
(3) by the mixing in described step (2) and dry carbide slag powder at 100.0-350.0kgf/cm
2forming pressure under compression moulding pressurize 0.5-3.0min, dry 10.0-24.0h.As pressure 100.0-300.0kgf/cm
2, calcium oxide pelletizing heat-shock resistance improves along with the increase of pressure.When the dwell time is 0.5-3.0min, calcium oxide pelletizing heat-shock resistance improves along with the prolongation of dwell time.Be 10.0-24.0h when drying, calcium oxide pelletizing heat-shock resistance improves along with the prolongation of time of drying.
(4) by the dried carbide slag base substrate in described step (3) at CO
2in the atmosphere of concentration 10.0-25.0%, 450.0-650.0 DEG C is heated to and constant temperature preheating 15.0-45.0min with the temperature rise rate of 3.0-10.0 DEG C/min, be heated to 900.0-1150.0 DEG C with the temperature rise rate of 8.0-13.0 DEG C/min again and calcine 90.0-120.0min, finally obtaining calcium oxide pelletizing with the cooling of the rate of temperature fall of 8.0-15.0 DEG C/min.Work as CO
2gas concentration is 10.0-25.0%, and calcium oxide pelletizing heat-shock resistance is along with CO
2the increase of gas concentration and improving.When temperature rise rate is 3.0-5.0 DEG C/min, calcium oxide pelletizing heat-shock resistance reduces along with the increase of temperature rise rate.When preheating thermostat temperature is 450.0-650.0 DEG C, calcium oxide pelletizing heat-shock resistance improves along with the increase of thermostat temperature.When preheating constant temperature time is 15.0-45.0min, calcium oxide pelletizing heat-shock resistance improves along with the increase of constant temperature time.When calcining temperature is 900.0-1150.0 DEG C, calcium oxide pelletizing heat-shock resistance improves along with the increase of calcining temperature.When being upon calcination 90.0-120.0min, calcium oxide pelletizing heat-shock resistance improves along with the increase of calcination time.Calcinating system schematic diagram as shown in Figure 2.
The present invention has the following advantages compared with existing high-heat resistance shock resistant calcium oxide pelletizing process of preparing:
(1) obtain high-heat resistance shock resistant and take into account calcium oxide pellet strength, activity simultaneously
The present invention has successfully prepared high-heat resistance shock resistant calcium oxide pelletizing, efficiently solves pelletizing calcium oxide and is entering in rotary kiln, furnace of calcium carbide use procedure by the technical barrier being easy to efflorescence in chilling and anxious thermal shocking situation and bursting.900.0 DEG C of thermal shocks 5.0-10.0 strength degradation 6.0%-25.0%, obtains calcium oxide content 92.5% simultaneously, activity is greater than 390.0ml, calcium oxide pelletizing that agglomerate intensity is greater than 4.6MPa.
(2) in-situ preparation pore-forming material
This regulate and control method make use of calcium hydroxide and to calcine in carbon dioxide atmosphere easily and carbon dioxide reaction generates the unstable characteristic of calcium carbonate, utilize the calcium carbonate original position of carbonization to produce pore-forming material, in decomposition course, produce carbon dioxide effusion form a large amount of pores.Pore structure inhibits thermal crack to expand on the one hand, effectively improves thermal conductivity on the other hand, is conducive to the large hot-fluid in local and disperses.
(3) carbide slag is main raw material(s), turns waste into wealth
Calcium oxide pelletizing of the present invention is main raw material with carbide slag, is recycling in calcium carbide and produces, form the circulation of the recycling of calcium carbide-carbide slag-lime-calcium carbide.The utilization ratio of carbide slag in calcium oxide agglomerate reaches 88-94%, not only effectively solves the problem of environmental pollution in calcium carbide process PVC production process but also reduce starting material input cost.
(4) operating procedure is simple, equipment is ripe
Operating procedure of the present invention is simple, can directly use the Thermal Equipment as the lime such as rotary kiln, burning clinker of cement to complete, technology maturation, be easy to realize large production.
Accompanying drawing explanation
Fig. 1 is a kind of high-heat resistance shock resistant calcium oxide pelletizing and preparation method's process flow sheet;
Fig. 2 is pelletizing Temperature Programmed Processes schematic diagram in calcine by steps process.
Embodiment
The present invention is introduced in detail below in conjunction with drawings and the specific embodiments.But following embodiment is only limitted to explain the present invention, and protection scope of the present invention should comprise the full content of claim, is not limited only to the present embodiment.And the present invention passes through embodiment below, those skilled in the art are all the elements that can realize the claims in the present invention record completely.
Embodiment 1
The technology of the present invention solution: a kind of high-heat resistance shock resistant calcium oxide pelletizing and preparation method, comprise the following steps:
(1) Ca (OH)
2it is 60.0-150.0 μm that the carbide slag powder that purity is greater than 90.0% is milled to granularity, and three kinds of granularity (60-90 μm: 90-120 μm: 120-150 μm) quality proportionings are respectively 4.0:2.0:4.0.Calcium oxide pelletizing heat-shock resistance increases with carbide slag powder granularity and reduces.
(2) H of 5.0% will be added in carbide slag powder pretreated in described step (1)
2o is as binding agent and mix, and calcium oxide pelletizing heat-shock resistance increases with water add-on and improves.
(3) by the mixing in described step (2) and dry carbide slag powder at 100.0kgf/cm
2forming pressure under compression moulding pressurize 0.5min, dry 10.0h.As pressure 100.0kgf/cm
2, calcium oxide pelletizing heat-shock resistance improves along with the increase of pressure.When the dwell time is 0.5min, calcium oxide pelletizing heat-shock resistance improves along with the prolongation of dwell time.Be 10.0h when drying, calcium oxide pelletizing heat-shock resistance improves along with the prolongation of time of drying.
(4) by the dried carbide slag base substrate in described step (3) at CO
2in the atmosphere of concentration 10.0%, 450.0 DEG C are heated to and constant temperature preheating 15.0min with the temperature rise rate of 3.0 DEG C/min, be heated to 900.0 DEG C with the temperature rise rate of 8.0 DEG C/min again and calcine 90.0min, finally obtaining calcium oxide pelletizing with the cooling of the rate of temperature fall of 8.0 DEG C/min.Work as CO
2gas concentration is 10.0%, and calcium oxide pelletizing heat-shock resistance is along with CO
2the increase of gas concentration and improving.When temperature rise rate is 3.0 DEG C/min, calcium oxide pelletizing heat-shock resistance reduces along with the increase of temperature rise rate.When preheating thermostat temperature is 450.0 DEG C, calcium oxide pelletizing heat-shock resistance improves along with the increase of thermostat temperature.When preheating constant temperature time is 15.0min, calcium oxide pelletizing heat-shock resistance improves along with the increase of constant temperature time.When calcining temperature is 900.0 DEG C, calcium oxide pelletizing heat-shock resistance improves along with the increase of calcining temperature.When being upon calcination 90.0min, calcium oxide pelletizing heat-shock resistance improves along with the increase of calcination time.
Product calcium oxide pelletizing 900.0 DEG C of thermal shocks 5.0 strength degradation 15.0% that the present invention prepares, calcium oxide content 90.5%, activity are greater than 370.0ml, agglomerate intensity is greater than 2.8MPa.Carbide slag utilization ratio 89-91%.
Embodiment 2
The technology of the present invention solution: a kind of high-heat resistance shock resistant calcium oxide pelletizing and preparation method, comprise the following steps:
(1) Ca (OH)
2it is 60.0-150.0 μm that the carbide slag powder that purity is greater than 92.4% is milled to granularity, and three kinds of granularity (60-90 μm: 90-120 μm: 120-150 μm) quality proportionings are respectively 4.0:4.0:2.0.Calcium oxide pelletizing heat-shock resistance increases with carbide slag powder granularity and reduces.
(2) H of 10.0% will be added in carbide slag powder pretreated in described step (1)
2o is as binding agent and mix, and calcium oxide pelletizing heat-shock resistance increases with water add-on and improves.
(3) by the mixing in described step (2) and dry carbide slag powder at 250.0kgf/cm
2forming pressure under compression moulding pressurize 2.5min, dry 20.0h.As pressure 250.0kgf/cm
2, calcium oxide pelletizing heat-shock resistance improves along with the increase of pressure.When the dwell time is 2.5min, calcium oxide pelletizing heat-shock resistance improves along with the prolongation of dwell time.Be 20.0h when drying, calcium oxide pelletizing heat-shock resistance improves along with the prolongation of time of drying.
(4) by the dried carbide slag base substrate in described step (3) at CO
2in the atmosphere of concentration 15.0%, 550.0 DEG C are heated to and constant temperature preheating 30.0min with the temperature rise rate of 4.0 DEG C/min, be heated to 1000.0 DEG C with the temperature rise rate of 7.0 DEG C/min again and calcine 100.0min, finally obtaining calcium oxide pelletizing with the cooling of the rate of temperature fall of 7.0 DEG C/min.Work as CO
2gas concentration is 15.0%, and calcium oxide pelletizing heat-shock resistance is along with CO
2the increase of gas concentration and improving.When temperature rise rate is 4.0 DEG C/min, calcium oxide pelletizing heat-shock resistance reduces along with the increase of temperature rise rate.When preheating thermostat temperature is 550.0 DEG C DEG C, calcium oxide pelletizing heat-shock resistance improves along with the increase of thermostat temperature.When preheating constant temperature time is 30.0min, calcium oxide pelletizing heat-shock resistance improves along with the increase of constant temperature time.When calcining temperature is 1000.0 DEG C, calcium oxide pelletizing heat-shock resistance improves along with the increase of calcining temperature.When being upon calcination 100.0minmin, calcium oxide pelletizing heat-shock resistance improves along with the increase of calcination time.
Product calcium oxide pelletizing 900.0 DEG C of thermal shocks 5.0 strength degradation 7.0% that the present invention prepares, calcium oxide content 92.5%, activity are greater than 380.0ml, agglomerate intensity is greater than 4.8MPa.Carbide slag utilization ratio is 90-93%.
Embodiment 3
The technology of the present invention solution: a kind of high-heat resistance shock resistant calcium oxide pelletizing and preparation method, comprise the following steps:
(1) Ca (OH)
2it is 60.0-150.0 μm that the carbide slag powder that purity is greater than 94.0% is milled to granularity, and three kinds of granularity (60-90 μm: 90-120 μm: 120-150 μm) quality proportionings are respectively 6.0:2.0:2.0.Calcium oxide pelletizing heat-shock resistance increases with carbide slag powder granularity and reduces.
(2) H of 15.0% will be added in carbide slag powder pretreated in described step (1)
2o is as binding agent and mix, and calcium oxide pelletizing heat-shock resistance increases with water add-on and improves.
(3) by the mixing in described step (2) and dry carbide slag powder at 350.0kgf/cm
2forming pressure under compression moulding pressurize 3.0min, dry 24.0h.As pressure 300.0kgf/cm
2, calcium oxide pelletizing heat-shock resistance improves along with the increase of pressure.When the dwell time is 3.0min, calcium oxide pelletizing heat-shock resistance improves along with the prolongation of dwell time.Be 24.0h when drying, calcium oxide pelletizing heat-shock resistance improves along with the prolongation of time of drying.
(4) by the dried carbide slag base substrate in described step (3) at CO
2in the atmosphere of concentration 25.0%, 650.0 DEG C are heated to and constant temperature preheating 45.0min with the temperature rise rate of 10.0 DEG C/min, be heated to 1150.0 DEG C with the temperature rise rate of 13.0 DEG C/min again and calcine 120.0min, finally obtaining calcium oxide pelletizing with the cooling of the rate of temperature fall of 15.0 DEG C/min.Work as CO
2gas concentration is 25.0%, and calcium oxide pelletizing heat-shock resistance is along with CO
2the increase of gas concentration and improving.When temperature rise rate is 5.0 DEG C/min, calcium oxide pelletizing heat-shock resistance reduces along with the increase of temperature rise rate.When preheating thermostat temperature is 650.0 DEG C, calcium oxide pelletizing heat-shock resistance improves along with the increase of thermostat temperature.When preheating constant temperature time is 45.0min, calcium oxide pelletizing heat-shock resistance improves along with the increase of constant temperature time.When calcining temperature is 1150.0 DEG C, calcium oxide pelletizing heat-shock resistance improves along with the increase of calcining temperature.When being upon calcination 120.0min, calcium oxide pelletizing heat-shock resistance improves along with the increase of calcination time.
Product calcium oxide pelletizing 900.0 DEG C of thermal shocks 5.0 strength degradation 25.0% that the present invention prepares, calcium oxide content 93.5%, activity are greater than 390.0ml, agglomerate intensity is greater than 4.6MPa.Carbide slag utilization ratio carbide slag utilization ratio 90-93%.
It should be noted that, according to the various embodiments described above of the present invention, those skilled in the art are the four corners that can realize independent claim of the present invention and appurtenance completely, implementation procedure and the same the various embodiments described above of method; And non-elaborated part of the present invention belongs to techniques well known.
The above; be only part embodiment of the present invention, but protection scope of the present invention is not limited thereto, any those skilled in the art are in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.
Claims (3)
1. a high-heat resistance shock resistant calcium oxide pelletizing, it is characterized in that: described calcium oxide pelletizing is prepared from by large Industrial Solid Waste carbide slag, carbide slag utilization ratio 88-94%, described carbide slag raw material is made up of the carbide slag that three kinds of granularities are different, and the weight proportion between three kinds of carbide slag grain graininess is: (60-90 μm: 90-120 μm: 120-150 μm) is respectively (4-6:2-4:2-4);
Described calcium oxide pelletizing porosity is 71-82%, and pore diameter range is 750-890nm, and thermal expansivity is ± 20-31 μm.
2. high-heat resistance shock resistant calcium oxide pelletizing according to claim 1, it is characterized in that: described calcium oxide pelletizing with the room temperature temperature difference be 500.0-1100.0 DEG C, cold cycling 5.0-10.0 time time, strength degradation 6.0%-25.0%, simultaneous oxidation calcium contents is 90.5-95.0%, activity is 350.0-400.0ml, agglomerate intensity is 2.5-4.6MPa.
3. a preparation method for high-heat resistance shock resistant calcium oxide pelletizing, is characterized in that comprising the following steps:
(1) carbide slag powder pre-treatment, by Ca (OH)
2it is 60.0-150.0 μm that the carbide slag powder that purity is greater than 91.0-94.0% is milled to granularity, and the weight proportion between three kinds of carbide slag grain graininess is: (60-90 μm: 90-120 μm: 120-150 μm) is respectively (4-6:2-4:2-4);
(2) H of 5.0-15.0% is added in carbide slag powder pre-treatment in described step (1) obtained
2o also mixes;
(3) by the carbide slag powder of mixing in described step (2) at 100.0-350.0kgf/cm
2forming pressure under compression moulding pressurize 0.5-3.0min, then at 100-120 DEG C of dry 10.0-24.0h;
(4) by the dried carbide slag base substrate in described step (3) at CO
2concentration is that the atmosphere of 10.0-25.0% is heated to 450.0-650.0 DEG C and constant temperature preheating 15.0-45.0min with the temperature rise rate of 3.0-10.0 DEG C/min, be heated to 900.0-1150.0 DEG C with the temperature rise rate of 8.0-15.0 DEG C/min again and calcine 90.0-120.0min, finally cooling to room temperature with the furnace with the rate of temperature fall of 8.0-15.0 DEG C/min and obtain calcium oxide pelletizing.
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| CN111485063B (en) * | 2020-06-06 | 2021-09-17 | 内蒙古铧钰环保材料有限公司 | High-efficiency utilization process of aluminum ash in electrolytic aluminum plant |
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